EP0927886A1 - Verfahren zur Detektion und Charakterisierung von Kohlenwasserstoffen in unterirdischen Lagerstätten - Google Patents

Verfahren zur Detektion und Charakterisierung von Kohlenwasserstoffen in unterirdischen Lagerstätten Download PDF

Info

Publication number
EP0927886A1
EP0927886A1 EP98403301A EP98403301A EP0927886A1 EP 0927886 A1 EP0927886 A1 EP 0927886A1 EP 98403301 A EP98403301 A EP 98403301A EP 98403301 A EP98403301 A EP 98403301A EP 0927886 A1 EP0927886 A1 EP 0927886A1
Authority
EP
European Patent Office
Prior art keywords
sample
hydrocarbons
fluorescence
quotient
value
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP98403301A
Other languages
English (en)
French (fr)
Other versions
EP0927886B1 (de
Inventor
Claudine Boehm
Jean Bernard Berrut
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Elf Exploration Production SAS
Original Assignee
Elf Exploration Production SAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Elf Exploration Production SAS filed Critical Elf Exploration Production SAS
Publication of EP0927886A1 publication Critical patent/EP0927886A1/de
Application granted granted Critical
Publication of EP0927886B1 publication Critical patent/EP0927886B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/24Earth materials
    • G01N33/241Earth materials for hydrocarbon content
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00Features of devices classified in G01N21/00
    • G01N2201/12Circuits of general importance; Signal processing
    • G01N2201/129Using chemometrical methods

Definitions

  • the present invention relates to research and the exploitation of formation hydrocarbons.
  • Drilling operations for research of hydrocarbons in underground formations are long and expensive.
  • a way to reduce the duration and cost of these operations is the optimization of the detection of formation hydrocarbons in all drilling conditions.
  • This optimization consists in ensuring the recognition of all impregnated and oriented rocks the test program so as to precisely define the areas to be tested.
  • the object of the present invention is precisely to remedy these drawbacks and provide a method of detection and characterization of hydrocarbons training.
  • This process can be used in the laboratory and on oilfield drilling sites
  • the hydrocarbon solvent is preferably cyclohexane.
  • the band L of wavelengths is comprised of preferably substantially between 280 and 500 nanometers
  • the value x corresponds to the mark of a length wave ⁇ x substantially equal to 367 nanometers, representative of the cut between the spectra emitted on the one hand, by the monoaromatic, diaromatic and part hydrocarbons triaromatics and on the other hand, by hydrocarbons polyaromatics.
  • a low value of the fluorescence quotient of the material sample is significant of the presence of light hydrocarbons in said sample and a value high is significant of the presence of hydrocarbons heavy.
  • the method of the invention consists in taking a series of samples of material at different depths during drilling, at determine the fluorescence quotient and the emission flux of each sample and then plotting the curves representative of said fluorescence quotient and of said flux emission as a function of depths, variations in fluorescence and emission flux quotient, allowing respectively to characterize the nature of the elements fluorescent and appreciate the importance of concentration of said elements in the series of material samples.
  • the method of the invention consists in comparing the fluorescence quotient at least one material sample, at the quotient of fluorescence of at least one product sample of reference determined in the same way as the quotient of fluorescence of the material sample.
  • the reference product sample consists of a mud sample taken during drilling.
  • a fluorescence quotient value of a material sample close to the value of the quotient of fluorescence of the mud sample taken during drilling, is significant of the absence of hydrocarbons from training in the material sample and a value different, is significant of a presence if moreover the emission flux value of the material sample is high.
  • the method of the invention is used to detect and characterize hydrocarbons training.
  • This process consists of taking from different depths during drilling, part of the cuttings for constitute a series of material samples, representative of the rocks crossed.
  • each sample takes a determined quantity of material to be analyzed, extract using a known amount of cyclohexane, the hydrocarbons contained in the quantity of material to be analyzed from each sample to constitute a series initial extracts. These initial extracts are then diluted by a dilution factor d to obtain extracts final.
  • the factor d is determined experimentally for each sample so that the concentrations in hydrocarbons in the final extracts are located in the measuring range of the spectrofluorimeter which will be used by the following.
  • cyclohexane as a solvent for hydrocarbons is particularly interesting because it favors the extraction of polyaromatized compounds representative of recoverable formation hydrocarbons while aliphatic solvents are more restrictive and that chlorinated solvents also dissolve heavy and polar hydrocarbons which are less mobile and therefore more difficult to recover.
  • Each final extract is introduced into a spectrofluorimeter where it is excited by radiation ultraviolet wavelength equal to 265 nanometers.
  • This wavelength is chosen due to the known property that the irradiated hydrocarbons have to emit by fluorescence. This wavelength also has the advantage to maximize the fluorescence emission of hydrocarbons from formation and minimize that of the hydrocarbons contained in oil sludge.
  • the intensity of the radiation emitted by fluorescence by each final extract is recorded using the spectrofluorimeter on an L band of wavelengths significant between 288 and 498 nanometers.
  • L ( ⁇ ) such as that of FIG. 1 which represents the variations in the intensity of the radiation emitted by fluorescence as a function of the emission wavelength ⁇ .
  • the shape of this spectrum is the direct signature of nature fluid that permeates the rocks in the area in which the material sample was taken.
  • the FLUXp value is proportional to the concentration of fluorescent elements including in particular the formation hydrocarbons, contained in the sample of material, taken at depth p.
  • the fluorescence quotient of the sample of material is equal to the ratio of areas 3 and 4 in Figure 2.
  • fluorescence QFp quotient of a sample is different from the fluorescence QFb quotient of mud and if the value FLUXp of the emission flux of the same sample is large, it means that hydrocarbons from training are present at depth p.
  • the values of the emission flows at the different depths reflect the hydrocarbon concentration of formation present in the rocks crossed.
  • the method of the invention allows relatively characterize the nature of the fluorescent elements extracts from material samples taken at different depths and appreciate the concentration in all drilling conditions and particularly in the case of oil mud drilling.
  • the liquid part of this set constitutes the extract initial oil.
  • This solution constitutes the final extract that partially transfers into the cell of a spectrofluorimeter LS50B model manufactured by PERKIN ELMER.
  • the final extract is excited by radiation ultraviolet wavelength equal to 265 nanometers bandwidth 15 nanometers.
  • the raw spectrum of the radiation emitted by fluorescence with the final extract i.e. records the values of the intensity of the radiation emitted in the L band of wavelength 288 to 498 nm at speed of 120 nm / minutes, through a window with a width of 5 nm band.
  • the recorded raw spectrum is then transferred to a DIGITAL 466 microcomputer connected to the spectrofluorimeter.
  • An analytical blank is performed by applying the same procedure as above without material sample.
  • P means depth at which corresponds to the taking of the sample during drilling and NS not significant value.
  • the very low value of the flux for the depth of 2,025.50 m means that if there is oil at this depth they are in very small quantity.
  • Zone A flux values on average plus higher than that of the area flows a reflect a more high concentration of hydrocarbons in zone A than in zone B.

Landscapes

  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • General Physics & Mathematics (AREA)
  • General Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Medicinal Chemistry (AREA)
  • Food Science & Technology (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Remote Sensing (AREA)
  • Geology (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
EP98403301A 1997-12-30 1998-12-24 Verfahren zur Detektion und Charakterisierung von Kohlenwasserstoffen in unterirdischen Lagerstätten Expired - Lifetime EP0927886B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9716711 1997-12-30
FR9716711A FR2773219B1 (fr) 1997-12-30 1997-12-30 Procede de detection et de caracterisation d'hydrocarbures de formation

Publications (2)

Publication Number Publication Date
EP0927886A1 true EP0927886A1 (de) 1999-07-07
EP0927886B1 EP0927886B1 (de) 2003-09-17

Family

ID=9515305

Family Applications (1)

Application Number Title Priority Date Filing Date
EP98403301A Expired - Lifetime EP0927886B1 (de) 1997-12-30 1998-12-24 Verfahren zur Detektion und Charakterisierung von Kohlenwasserstoffen in unterirdischen Lagerstätten

Country Status (7)

Country Link
US (1) US6271518B1 (de)
EP (1) EP0927886B1 (de)
CA (1) CA2256082C (de)
DE (1) DE69818216T2 (de)
ES (1) ES2206874T3 (de)
FR (1) FR2773219B1 (de)
NO (1) NO327823B1 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2554654C1 (ru) * 2014-01-29 2015-06-27 муниципальное бюджетное образовательное учреждение "Общеобразовательное учреждение лицей N 1" Способ анализа образцов горных пород

Families Citing this family (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU2002227772B2 (en) * 2001-01-23 2005-07-07 Commonwealth Scientific And Industrial Research Organisation Oil reservoirs
US7173242B2 (en) * 2001-01-23 2007-02-06 Commonwealth Scientific And Industrial Research Organisation Method for determining whether a rock is capable of functioning as an oil reservoir
US7501285B1 (en) * 2004-09-16 2009-03-10 Marathon Ashland Petroleum Llc Detection and classification of heavy hydrocarbon contamination in refinery process streams via spectrofluorometry
FR2883916B1 (fr) * 2005-04-04 2007-07-06 Geoservices Procede de determination de la teneur en au moins un gaz donne dans une boue de forage, dispositif et installation associes
CN101689102B (zh) * 2007-02-16 2014-01-29 沙特阿拉伯石油公司 测定储集岩中有机物质体积的方法
CN107167400B (zh) * 2017-05-03 2021-11-09 黑龙江八一农垦大学 一种石油包裹体中原油密度的检测方法
US10696906B2 (en) 2017-09-29 2020-06-30 Marathon Petroleum Company Lp Tower bottoms coke catching device
US12000720B2 (en) 2018-09-10 2024-06-04 Marathon Petroleum Company Lp Product inventory monitoring
US12031676B2 (en) 2019-03-25 2024-07-09 Marathon Petroleum Company Lp Insulation securement system and associated methods
US11975316B2 (en) 2019-05-09 2024-05-07 Marathon Petroleum Company Lp Methods and reforming systems for re-dispersing platinum on reforming catalyst
US11124714B2 (en) 2020-02-19 2021-09-21 Marathon Petroleum Company Lp Low sulfur fuel oil blends for stability enhancement and associated methods
US11898109B2 (en) 2021-02-25 2024-02-13 Marathon Petroleum Company Lp Assemblies and methods for enhancing control of hydrotreating and fluid catalytic cracking (FCC) processes using spectroscopic analyzers
US11905468B2 (en) 2021-02-25 2024-02-20 Marathon Petroleum Company Lp Assemblies and methods for enhancing control of fluid catalytic cracking (FCC) processes using spectroscopic analyzers
US11702600B2 (en) 2021-02-25 2023-07-18 Marathon Petroleum Company Lp Assemblies and methods for enhancing fluid catalytic cracking (FCC) processes during the FCC process using spectroscopic analyzers
US20220268694A1 (en) 2021-02-25 2022-08-25 Marathon Petroleum Company Lp Methods and assemblies for determining and using standardized spectral responses for calibration of spectroscopic analyzers
US11692141B2 (en) 2021-10-10 2023-07-04 Marathon Petroleum Company Lp Methods and systems for enhancing processing of hydrocarbons in a fluid catalytic cracking unit using a renewable additive
US11802257B2 (en) 2022-01-31 2023-10-31 Marathon Petroleum Company Lp Systems and methods for reducing rendered fats pour point

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2142955A (en) * 1983-07-06 1985-01-30 Nl Petroleum Services Improvements in or relating to the testing for the presence of native hydrocarbons down a borehole
US4783416A (en) * 1987-05-08 1988-11-08 Shell Oil Company Analytical method to determine the unwashed gum content in a gasoline boiling hydrocarbon
US4814614A (en) * 1987-05-11 1989-03-21 Mobil Oil Corporation Method for characterizing oil-bearing inclusions via fluorescence microspectrophotometry
EP0342869A1 (de) * 1988-05-14 1989-11-23 Exxon Research And Engineering Company Chromatographische Analyse von Kohlenwasserstoffölen
US4959549A (en) * 1986-11-28 1990-09-25 Commonwealth Scientific And Industrial Research Organisation Determination of properties of coal

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4988446A (en) 1988-05-14 1991-01-29 Exxon Research And Engineering Company Method for spectroscopic analysis of hydrocarbons
US5076909A (en) 1988-05-14 1991-12-31 Exxon Research And Engineering Company Method for refining or upgrading hydrocarbons with analysis

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2142955A (en) * 1983-07-06 1985-01-30 Nl Petroleum Services Improvements in or relating to the testing for the presence of native hydrocarbons down a borehole
US4959549A (en) * 1986-11-28 1990-09-25 Commonwealth Scientific And Industrial Research Organisation Determination of properties of coal
US4783416A (en) * 1987-05-08 1988-11-08 Shell Oil Company Analytical method to determine the unwashed gum content in a gasoline boiling hydrocarbon
US4814614A (en) * 1987-05-11 1989-03-21 Mobil Oil Corporation Method for characterizing oil-bearing inclusions via fluorescence microspectrophotometry
EP0342869A1 (de) * 1988-05-14 1989-11-23 Exxon Research And Engineering Company Chromatographische Analyse von Kohlenwasserstoffölen

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2554654C1 (ru) * 2014-01-29 2015-06-27 муниципальное бюджетное образовательное учреждение "Общеобразовательное учреждение лицей N 1" Способ анализа образцов горных пород

Also Published As

Publication number Publication date
NO327823B1 (no) 2009-10-05
NO986175D0 (no) 1998-12-29
CA2256082C (fr) 2006-06-27
DE69818216T2 (de) 2004-07-08
FR2773219B1 (fr) 2000-02-18
EP0927886B1 (de) 2003-09-17
FR2773219A1 (fr) 1999-07-02
DE69818216D1 (de) 2003-10-23
US6271518B1 (en) 2001-08-07
ES2206874T3 (es) 2004-05-16
NO986175L (no) 1999-07-01
CA2256082A1 (fr) 1999-06-30

Similar Documents

Publication Publication Date Title
EP0927886B1 (de) Verfahren zur Detektion und Charakterisierung von Kohlenwasserstoffen in unterirdischen Lagerstätten
FR2556465A1 (fr) Perfectionnements relatifs aux essais pratiques en vue de determiner la presence d'hydrocarbures naturels au fond d'un trou de sondage
EP0794432B1 (de) Verfahren zur Feststellung des Ölgehaltes einer unterirdischen Formation mittels Bohrklein
EA013889B1 (ru) Способ и устройство для определения состава флюида в скважине
FR2806159A1 (fr) Procede et dispositif optique pour la mesure non intrusive de la temperature dans un liquide en ecoulement
US20220178825A1 (en) Apparatus and method for determination of banned substances
EP0691540A1 (de) Verbessertes Verfahren zur schnellen Auswertung von mindestens einer petrologischen Eigenschaft einer Steinprobe und Anwendung desselben bei Schweröl enthaltenden Schichten
US20040099804A1 (en) Oil reservoirs
FR2855267A1 (fr) Affinement de signaux pour l'analyse optique de fluides
CN108489952B (zh) 三维荧光光谱结合二次微分检测水体溶解性有机物的方法
CN107255629A (zh) 一种食品中罗丹明b快速检测方法
FR2815074A1 (fr) Methode d'analyse et de mesures chimique et isotopique sur des constituants transportes par un fluide de forage
EP2307877B1 (de) Verfahren zum nachweis funktioneller carbonsäuregruppen
FR3036430A1 (de)
FR2561387A1 (fr) Procede de dosage de traces d'uranium en solution par spectrofluorimetrie a resolution temporelle
FR3062917A1 (fr) Analyse de particules metalliques dans des materiaux d'excavation
RU2629839C1 (ru) Способ определения содержания пальмового масла в молоке
WO2014184498A1 (fr) Procédé d'évaluation par biodosimétrie de la dose d'irradiation reçue par un individu ayant été soumis a un rayonnement ionisant
CN1073706C (zh) 一种石油荧光光谱录井仪
RU2554654C1 (ru) Способ анализа образцов горных пород
Cheng et al. Coumarin 6 staining method to detect microplastics
RU2663417C1 (ru) Способ подбора кислотного состава для интенсификации добычи нефти
EP3030909A1 (de) Verfahren und vorrichtung zur herstellung eines zellbehälters mit mittel zur voranalyse einer entnommenen probe
Azcue et al. Effects of centrifugation speed on measurements of thallium in sediment pore water
FR2983898A1 (fr) Procede de surveillance d'un site de stockage geologique de gaz au moyen de mesures de ph par fluorescence

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 19990104

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): DE ES GB IT NL

AX Request for extension of the european patent

Free format text: AL;LT;LV;MK;RO;SI

AKX Designation fees paid

Free format text: DE ES GB IT NL

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): DE ES GB IT NL

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

Free format text: NOT ENGLISH

REF Corresponds to:

Ref document number: 69818216

Country of ref document: DE

Date of ref document: 20031023

Kind code of ref document: P

GBT Gb: translation of ep patent filed (gb section 77(6)(a)/1977)

Effective date: 20031110

REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2206874

Country of ref document: ES

Kind code of ref document: T3

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed

Effective date: 20040618

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: NL

Payment date: 20171124

Year of fee payment: 20

Ref country code: DE

Payment date: 20171120

Year of fee payment: 20

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: IT

Payment date: 20171120

Year of fee payment: 20

Ref country code: GB

Payment date: 20171121

Year of fee payment: 20

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: ES

Payment date: 20180103

Year of fee payment: 20

REG Reference to a national code

Ref country code: DE

Ref legal event code: R071

Ref document number: 69818216

Country of ref document: DE

REG Reference to a national code

Ref country code: NL

Ref legal event code: MK

Effective date: 20181223

REG Reference to a national code

Ref country code: GB

Ref legal event code: PE20

Expiry date: 20181223

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF EXPIRATION OF PROTECTION

Effective date: 20181223

REG Reference to a national code

Ref country code: ES

Ref legal event code: FD2A

Effective date: 20200902

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: ES

Free format text: LAPSE BECAUSE OF EXPIRATION OF PROTECTION

Effective date: 20181225